反応 #9571

ord-85819ad6c6834adb8e5accf545355994

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    温度was heated
  2. 2
    温度at reflux overnight
  3. 3
    濃縮The reaction mixture was concentrated under reduced pressure
  4. 4
    その他the residue was purified by HPFC (
  5. 5
    洗浄eluting with chloroform

実験手順

A mixture of 5-bromo-N4-(2-methylpropyl)quinoline-3,4-diamine (1.0 g, 3.4 mmol), triethyl orthoformate (0.9 mL, 5 mmol), and pyridine hydrochloride (117 mg, 1.0 mmol) in acetonitrile (17 mL) was heated at reflux overnight. The reaction mixture was concentrated under reduced pressure, and the residue was purified by HPFC (eluting with chloroform:CMA in a gradient from 100:0 to 70:30) to provide 9-bromo-1-(2-methylpropyl)-1H-imidazo[4,5-c]quinoline as a dark oil.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US07091214B2uspto-grants-2006_08